of petit-quevilly



Feb. 19 1924. 1,484.587`

L. E. M. TREvqux l PROCESS AND APPARATUS FOR THE CONTINUOUS zRlODUCTION 0F SULPHATE-S Filed May 24.5!1921 2 sheets-sheet 1 Feb. I9 1924.

L. E. M. TREVOUX PROCESS AND APPARATUS FOR THE CONTINUOUS PRODUCTION OF SULPHATES Filed May 24. 1921 2 Sheets-Sheet 2 Patented Feb. 19, 1924.

UNITED STATES PATENT oFFicE.

LAURENT MILE' MARIE TREVOUX, 0F PETIT-QUEVILLY, FRANCE, ASSIGNOR TO LA SOCIETE ANONYME DE PRODUITS CHIMIQUES, ETABLISSEMENTS MALETEA, SIEGE SOCIAL, OF PETIT-GUEVILLY, FRANCE.

PROCESS AN D APPARATUS FOR TH CONTINUOUS PRODUCTION OF SULPHATES.

Application lled Hay 2li,

The known mechanical processes for thev production oi anhydrous sulphates, leading to an acid sulphate which is liquid in the wurm und to a solid anhydrous'sul .hatere only the reproduction of the con itions of hand labour which have existed for a. century, These Working conditions involve two distinct stages and relate to the handling of large quantities. The linking together of these two stages, liquid treatment and calciuing, can be realizedes systematically as possible. The consequence of all these types of furnaces is an emission of :gasrvarymg within wide. limits and a' considerable amount of condensation corresponding to these variations in emission.

It-is -true that ii. process, that of the Farb` werke vorm. Meister, Lucius and Bruning, of Hochst, is supposed -to be continuous, but in reality the only continuous port is the production of acid sodium sulphate NeHSO which does not present any ditiiculty. In

reality the second stage comprises complex operations of coolin the acid sul hate, crushing, mixing it with salt and fina 1y introducin it in a continuous .furnace which calcines t ie intimate mixture, and discharges it in u continuous mnner nt the bottom 0f the furnace.

The object of the present invention is based on the division o the work into three V stages which are all continuous and proceed in uninterrupted succession.

The first sta, e effects the continuous formation of aci sodium sulphate, the methodic introduction of sulfuric acid and salt -in the desired proportions in the interior of un ulrendy liquid mass of acid Sodium sul# phute which serves as a heat carrier and .eiiects the rapid transformation of the mixture of sulfuric acid and sodium Vchloride 1921. Serial No. 472,231.

charged into the mixer used for the third' st alettre third stage, the mixture of ecid sodium sulphate and salt, the original constituents of which have already partly reacted on one another, is comp etely transformed into sodium sulphate and hydrochloric scid in a mixing and cslcining furnace und discharged in a Continous manner from the bottom.

'These three stages must loe-carried out at suitable temperatures carefully re in view of the reactions to be obtained in. each stage. The stages 1 and 2 moreover, necessitate the suitable regulation of the admission of the two initial constituents. of euch stage.

A` way of carrying out the invention has been represented by way of example in the accompanying drawings.

Fig. 1' is a longitudinal section of the furnace. v

Fig. 2 is a. transverse section. on line 2 2, Fig: 1, showing the proportioneting.r mixer in willich the second 'stage of `the reaction is effected.

Fig. 3 is a vertical section of said miner, but showing the mixer in opposite position from Fig. 1. l

Figs. 4 and 5 are sections on lines 4-4 and `5--5 of Fig. 3.

A is a vessel of cylindrical shape and which is prolonged in the upward direction by )lain walls. In this vessel revolves a pad le agittor D which is mounted on the lated vides the vessel into two unequal chambers and retards the passage of the bisnlfate from the large into the smaller chamber, in such a way that the bisulphate which is scooped out by a scoop F at each rotation of its shaft Q shall consist of Well formed liquid acid sulphate.

This vessel A is heated to a suitable tcmperature by means of gases supplied from a furnace or from a producer, which gases have previously heated the calciniug furnace C and the mixer B.

At each rotation of shaft Q, the scoop l" scoops in the rear chamber of the vessel A a quantity of acid sulphate large enough to fill an annular pan G, which plays the part of a measuring device, the excess liquid falling back into the rear chamber, As the rotation of the sh ft continues, the measured volume of liquifalls through the slot l in the side Wall of the pan G, into the torusshaped pocket H of the mixer B. A scraper 5 ensures the cleaning of thsiannular measuring vpan G; said `scraper being attached to a shaft, (l, as clearly shown in Fig. 3.

At the same time the quantity of sea salt corresponding,r to the quantity of arid sulphate discharged as aboveI described isadmitted through the tube 6. so that the two constituents are in the desired proportions for the third stage of the reaction to yield neutralwsulphate. As the rotation of the mixer B continues the reaction between the two constituents proceeds, being aided by the mixing paddles 7, which describe a swinging movement, until the mixture reachef` the opening 8 in the Q and falls into the axis of the caleining pan C. A scraper 9, also provided on thc shaft and preferably connepted with the first scraper 5, prevents the mixture from remaim ing in the pocket H, and the paddles Tmayv form integral parts of the scraper t).

The sooo F and the pockrt H of the mixer B are pre erably. integral y r'otherwise rigidly connected together (Fig. fi) and 'are mounted on shaft Q, which latter is made, hollow to permit the scraper shaft q to extend through it.

There may be any desired number of paddles and Scrapers, and they may either rotate or swing in order to properly ellect their purpose. In the event of their rotating` the hollow shaft Q which carries the, parts l5 and F must turn at a much slower speed than the shaft f] which -carries the paddles and Scrapers.

The mixture falling from the mixer R into the calcining 'pan C is taken by the rabbles L and is slowly conveyed from the centre to the periphery alon; r a spiralvpath, b v the usual means, in such a way that the mixture plogressively attains the desired temperature so that the reaction is complete and the hydrochloric acid is completely libperiphery of the pocket H,

regards the ortions disengaged in A.B and C respective y, or in common.

What I claim and desire to secure by Letters Patent is:-

1. The recess for t-he continuous production of su phates from chlorides and sulfuric acid, which comprises methodically introducing the desired .amounts of sulfuric acidand chloride within an already liquid mass of acid sulphate serving as a heat carrier, and assisting in the rapid transformation of the chloride into acid sulphate, thereu on adding an adequate amount of chlori e to a liquid portion of said acid sulphate formed! and intimately mixing to. transform the mixture into a pasty mass and finally transforming said pasty mass into neutral sulphate by calcining said pasty mass whilst constantly stirring.

Q. The process for the continuous production of sodium sulphate from sea salt and sulfuric acid, which comprises methodically introducing the desired amounts of sulfuric acid and sea salt Within an already liquid mass of acid sodium sulphate serving as a heat carrier, and assisting in the rapid transformation of the sea salt into acid sodium sulphate, thereupon add,- iug an adequate amount of sea salt to a. liquid portion of said acid sodium sulphate formed and intimately mixing to transform the mixture into a pasty mass and g finally transformingY said pasty mass into neutral sodium sulphate by calcining said pasty mass whilst constantly stirring.

3. The process for the continuous production of sulphates, which consists in effecting in a single. apparatus and in three stages the transformation of chloride and sulfuric acid into sulphate; a first stage effeeling iu a continuous manner the formation of the acid sulphate by the systematic addition of sulfuric acid and of said chlo ride in the desired pro ortionsV and their action within an alrea y liquid mass of acid sulphate, said mass serving as heaty carrier and assisting in the rapid formation of the acid sulphate: a second stage etfecting the intimate mixing of the already formed arid sulphate and of chloride, by taking a liquid portion from the mixer of the first stage. and adding an adequate amount of chloride from a continuous distributor, said mixture becoming transformed rapidly into a pasty mass; and a third stage in which the mixture of acid sulphate and clitoride of the second stage, discharged as soon as formed, is completely transformed into neutral sulphate, with the formation of hydrochloric acid, in a calcining pan which acts at the same time as a mixer.

The process for the continuous production of sodium sul hate, which consists in effecting in a singe apparatus and in three stages the transformation of sea salt and sulfuric acid into sulphate; a first stage effecting in a continuous manner the formation of the acid sodium sulphate by the systematic addition of sulphuric acid and of the sea salt in the desired proportions and their action Within an already liquid mass of acid sulphate, said mass serving as heat carrier and assisting in the rapid formation of the acid sodium sulphate; a second stage effecting the intimate mixing of the already formed acid sodium sulphate and of sea salt, by taking a liquid portion from the mixer of the first stage, and adding an adequate amount of sea salt from a continuous distributor, said mixture becoming transformed rapidly into a pasty mass; and a third stage 1n which the mixture of acid sodium sulphate and chloride of the second stage, discharged as soon as formed is com letely transformed into neutral sodium su phate, with the formation of hydrochloric acid, in a calcining 4pan which acts at the same time as a mixer.

5. A single apparatus for effecting the continuous production of sulphates from chlorides and sulfuric acid, comprising a vessel adapted to lbe heated; means for suppliving salt and liquid acid to the heated vesse means for mixing the salt and acid in said vessel; a second veel; mixing means therein' means for removing measured quantitles of the mixture from the first vessel and depositing them in the second vessel; means for supplying measured quantities of salt to the contents of the second vessel to be mixed therewith, said second vessel having means for discharging the mixture obtained therein; and means for heating and stirring the last named mixture and for continuously eil'ecting its conveyance and tin'al discharge.

6. A single apparatus for effecting the continuous production of sulphates from chlorides and sulfuric acid comprising a vessel adapted to be heated; a transverse vertical partition in said veel dividing the interior thereof into two compartments and having an opening at its bottom to provide communication between the compartments;

meansL for supplying salt and liquid acid to one compartment; mixing means in said compartment; a rotatable vessel exterior to the other compartment having a scoop connected to it for removing measured quantities of the mixture from that compartment and discharging them into the rotatable vessel; mixing means in said rotatable vesscl: means for supplying measured quanti-l tics of salt to the rotatable vessel for admixture with the contents thereof, said rotatable vessel havin means for discharging the mixture obtaine therein; and means for heating and stirring the last named mixture and for continuously effecting its conveyance and final discharge.

7. In an apparatus for producing sulphates from chlorides and sulfuric acid, the combination of *a rotatable mixing vessel having a scoop connected to it to pick up measured quantities of liquid and dlscharge them into the interior of the vessel; and mixing means within said vessel for acting on the liquid thereon.

8. In an apparatus for producin sulphates from chlorides land sulfuric acld, the combination of a rotatable mixing veel having connected to one side thereof a scoop to pick up measured quantities of liquid and discharge them into the interior of the vessel, said vessel also having an outlet for the liquid which is located at a point remote from the mouth ofthe scoop; andA mixing means Within said vessel for acting on the liquid therein.

9. In an apparatus for producing sulphates from chlorides and su furie acid, the comfbination of a rotatable mixing vessel having a scoop connected to it to pick up measured quantities of liquid and discharge them into the interior of the vessel; a hol# low shaft on which said vessel is mounted to rotate'with the shaft; a shaft disposed within the first shaft and projecting into the interior of the vessel; and mixing means within said vessel secured to the projecting end of the second shafts y In testimony whereof I have signed this specification in the presence of two subscribing witnesses.

neveux, LAURENT naar mail.

Witnesses:

FERNAND DUFOUR, CHARLES LEON LoIsnL. 

